Detection of "Bath Salt" Synthetic Cathinones and Metabolites in Urine via DART-MS and Solid Phase Microextraction

Dania Al-Balaa, Ales Rajchl, Adéla Grégrová, Rudolf Sevčík and Helena Čízková

 

Department of Food Preservation, Institute of Chemical Technology, Prague, Czech Republic

 

To ensure that egg-containing products, such as dried eggs and egg pasta, conform to the technological and legislative requirements for egg content, methods are needed to determine the amount of cholesterol in such products. The conventional approach, direct saponification and hexane extraction followed by cholesterol determination by gas chromatography coupled to a flame ionization detector, is very time consuming. Therefore, we developed a rapid method on the basis of direct analysis in real time coupled to time-of-flight mass spectrometry. Samples were prepared simply by solvent extraction followed by extract filtration. The optimization of certain parameters, including the solvent used and direct analysis in real time ionization gas temperature, had a pronounced effect on the intensities of the produced ions, in particular, the molecular and dehydrated ions of cholesterol and its deuterated analog, cholesterol 2,2,3,4,4,6-d6, which was used as an internal standard. For the developed method, limits of detection and quantification were 0.03 and 0.05 mg/g, respectively. The results of the real samples were compared with those obtained using the conventional approach [limit of detection =0.002 mg/g and limit of quantification =0.05mg/g], and it was found that, although the results obtained using the conventional approach were more accurate, our developed method is much simpler and faster, where the time was dramatically reduced by 87% for executing a screening analysis.

Xue Li, Guangyue Hou, Junpeng Xing, Fengrui Song, Zhiqiang Liu, Shuying Liu 

  

Chemical Biology Laboratory and Changchun Center of Mass Spectrometry, Changchun Institute of Applied Chemistry, Chinese Academy of Sciences, Changchun, 130022; University of the Chinese Academy of Sciences, Beijing, 100039, China  

 

In the present work, direct analysis of real time ionization combined with multi-stage tandem mass spectrometry (DART-MSn) was used to investigate the metabolic profile of aconite alkaloids in rat intestinal bacteria. A total of 36 metabolites from three aconite alkaloids were identified by using DART-MSn, and the feasibility of quantitative analysis of these analytes was examined. Key parameters of the DART ion source, such as helium gas temperature and pressure, the source-to-MS distance, and the speed of the autosampler, were optimized to achieve high sensitivity, enhance reproducibility, and reduce the occurrence of fragmentation. The instrument analysis time for one sample can be less than 10 s for this method. Compared with ESI-MS and UPLC-MS, the DART-MS is more efficient for directly detecting metabolic samples, and has the advantage of being a simple, high-speed, high-throughput method.

IonSense, Inc. provides OpenSpot Mass Spectrometry™ solutions to the fields of food safety, forensics, drug development, and chemical analysis. We manufacture and develop direct analysis in real time (DART^®) technology licensed from JEOL USA, Inc. and atmospheric solids analysis probe (ASAP™) licensed from M&M Consulting.

DART and ASAP Sources are available for most commercial LC/MS systems.  Look here to see if your system is DART-ready.  And  check here to see if your system is ASAP-ready.

For your local representative, please see our distributor network.

Phone - 781.484.1043  | info@ionsense.com | http://www.ionsense.com